CN108517422A - A method of the high efficiente callback lithium from containing lithium more metal mixed solution - Google Patents
A method of the high efficiente callback lithium from containing lithium more metal mixed solution Download PDFInfo
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- CN108517422A CN108517422A CN201810300504.3A CN201810300504A CN108517422A CN 108517422 A CN108517422 A CN 108517422A CN 201810300504 A CN201810300504 A CN 201810300504A CN 108517422 A CN108517422 A CN 108517422A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of methods of the high efficiente callback lithium from containing lithium more metal mixed solution, include the following steps：(1) pH to 37 for adjusting more metal mixed solution containing lithium, then uses saponification organic phase extracting, obtains load organic phases and rich lithium raffinate；(2) the load organic phases acid adding back extraction processing, obtains strip liquor and back extraction organic phase；According to wherein species of metal ion and content, selective recovery utilizes the strip liquor, back extraction organic phase is washed, after saponification back to recycling in step (1)；(3) the rich lithium raffinate enters bipolar membrane electrodialysis system, output lithium hydroxide solution and acid solution after depth oil removal treatment；(4) lithium hydroxide solution obtains monohydrate lithium hydroxide powder and concentrated mother liquor through being concentrated by evaporation.Method of the invention it is achieved the disposable input of soda acid, whole process closed cycle, the production and operation is at low cost, process automation is controllable；Method using the present invention can make the rate of recovery containing lithium in the more metal mixed solution of lithium be more than 95%.
Description
Technical field
The invention belongs to nonferrous materials fields, more particularly to a kind of high efficiente callback from containing lithium more metal mixed solution
The method of lithium.
Background technology
Being flourished by new-energy automobile industry is influenced, and the market demand of the following lithium resource is by sustainable growth.To seize
The market share, each large enterprises in the whole world develop lithium resource exploitation business one after another, as ore carries lithium, salt lake carries lithium, old and useless battery recycling
Lithium etc..By the end of the end of the year 2016, global lithium salts production capacity has reached 19wt/a scales, and major product is lithium carbonate, and lithium hydroxide
Production capacity is only 6.4wt/a.
From the point of view of the extractive technique of lithium, either ore carries lithium, salt lake carries lithium or waste and old power battery carries lithium, current main
Waveguide technology is wet processing, i.e. Li enters solution together with other elements, the recycling extraction Li subsequently from solution.Therefore, may be used
The solution system that can relate to includes chloride system, sulfate system, the foreign metal ion that may relate to include mainly Ca,
Mg, Fe, Al, Cu, Ni, Co, Mn etc., lithium how is effectively extracted from containing the more metal mixed solution of lithium becomes current influence lithium recycling
Technical barrier.From the point of view of technology status at home and abroad, there are mainly two types of methods for the extraction containing lithium in the more metal mixed solution of lithium：One
It is chemical precipitation method, second is that solvent extraction；In terms of lithium product, currently mainly based on output lithium carbonate.Above two side
Method can realize the separation and recovery of Li in solution, but still have that recovery process is long, the Li rate of recovery is not high, lithium salts quality is irregular at present
Uneven, technique owes the problems such as environmental protection.
In downstream application field, as new-energy automobile steps up course continuation mileage and vehicle lightweight requirements, lithium
Electric positive electrode market is gradually tilted from LiFePO4 to trielement composite material, and the appearance of especially nickelic ternary material promotees
The market demand of lithium salts is set gradually to be shifted from lithium carbonate to lithium hydroxide.But from the point of view of current industry current situation, hydroxide
The industrial pattern of lithium is still pessimistic, just at present from the point of view of the production capacity adjustment of each relevant enterprise in the whole world, to 2019 end of the year whole world hydroxides
Lithium production capacity cannot meet tesla year by year high-volume caused by raw materials requirement.
Therefore, actively research containing the high efficiency extraction of lithium in the more metal mixed solution of lithium and prepares the production of high-quality lithium hydroxide
The core technology of product, effectively take into account the high yield of lithium, the high quality of product, technique it is environmentally protective, be lithium resource exploitation industry
Critical issue urgently to be resolved hurrily.
Invention content
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The method of kind high efficiente callback lithium from containing the more metal mixed solution of lithium.
In order to solve the above technical problems, technical solution proposed by the present invention is：
A method of the high efficiente callback lithium from containing lithium more metal mixed solution includes the following steps：
(1) pH to 3-7 for adjusting more metal mixed solution containing lithium, then uses saponification organic phase extracting impurity, is born
Carry organic phase and rich lithium raffinate；
(2) the load organic phases acid adding back extraction processing, obtains strip liquor and back extraction organic phase；The strip liquor is according to it
Middle species of metal ion and content, selective recovery utilize, organic phase is washed for back extraction, after saponification back in step (1) again
It utilizes；
(3) the rich lithium raffinate enters bipolar membrane electrodialysis system, output lithium hydroxide solution and acid solution；
(4) lithium hydroxide solution obtains monohydrate lithium hydroxide powder and concentrated mother liquor through being concentrated by evaporation.
Above-mentioned method, it is preferred that the saponification organic phase in step (1) refer to organic phosphates extractant through non-soda soap at
The organic phase obtained after reason.
Above-mentioned method, it is preferred that the organic phosphates extractant be selected from P204, P507, P229, Cyanex272,
At least one of Cyanex301, Cyanex471X, Cyanex921, Cyanex923.
Above-mentioned method, it is preferred that the saponification agent in the non-soda soap processing procedure is lithium sulfate, lithium hydroxide, carbon
It is one or more in the concentrated mother liquor generated in sour hydrogen lithium, lithium chloride and step (4)；It is further preferred that non-soda soap
The saponification agent used in processing procedure for the concentrated mother liquor that generates in step (4), LiOH a concentration of 20 in the concentrated mother liquor~
130g/L。
Above-mentioned method, it is preferred that the concentrated mother liquor of step (4) output is directly entered soap tank first order mixing chamber,
The saponification extraction raffinate of soap tank afterbody clarifying chamber returns in step (4) and is evaporated concentration.
Above-mentioned method, it is preferred that in the non-soda soap processing procedure, saponification is comparably O/A=1:1~1:10, it mixes
The conjunction time is 1~10min, and settling time is 1~30min, 2~10 grades of saponification series.Using such saponification process, can set
Change the H in extractant+, while not introducing other impurities ion again.
Above-mentioned method, it is preferred that solution pH adjusting agent is one kind in lithium hydroxide, sulfuric acid and hydrochloric acid in step (1)
Or it is a variety of；It is further preferred that pH adjusting agent is the lithium hydroxide solution or acid solution of output in step (3).Using such
Treatment process can fully realize the soda acid closed cycle of internal system.
Above-mentioned method, it is preferred that for load organic phases in the acid solution return to step (2) of output in step (3)
Back extraction.
Compared with the prior art, the advantages of the present invention are as follows：
(1) method using the present invention, the rate of recovery containing lithium in the more metal mixed solution of lithium are more than 95%.
(2) method of the invention, introduces non-soda soap abstraction technique, avoids the chemistry present in traditional chemical partition method
The problems such as reagent consumption is high, lithium resource entrainments at different levels disperse, while realizing the disposable input of soda acid, whole process closed cycle,
The production and operation is at low cost, process automation is controllable.
(3) method of the invention introduces the one-step method Forms Transformation that bipolar membrane electrodialysis technology realizes lithium, avoids causticization
Method prepares the problems such as alkaline consumption present in lithium hydroxide is high, lithium yield is low；Simultaneously saponification agent original is provided for the non-soda soap of back
Material not the case where additional chemical agent, realizes marketing one's own products for material inside processing system.
(4) method of the invention, technological process is simple, processing cost is low, three-waste free discharge.
(5) the method for the present invention can handle more metal mixed solution containing lithium of various various concentration contents, and technological adaptability is wide.
Description of the drawings
Fig. 1 is the technological process of the method for high efficiente callback lithium from containing lithium more metal mixed solution in the embodiment of the present invention 1
Figure.
Specific implementation mode
To facilitate the understanding of the present invention, it is done more entirely below in conjunction with Figure of description and preferred embodiment to inventing herein
Face meticulously describes, but protection scope of the present invention is not limited to following specific examples.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention's
Protection domain.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1：
A method of the high efficiente callback lithium from containing lithium more metal mixed solution, process flow chart is as shown in Figure 1, include
Following steps：
(1) organic extractant P204 carries out saponification process using the LiOH solution of a concentration of 120g/L, and O/A is compared in saponification
=1:2, incorporation time 10min, settling time 15min, saponification series are 2 grades, and organic phase saponification rate is 64%, more than saponification
Liquid enters step the evaporative concentration stage of saline of (5)；
(2) lithium hydroxide is added into lepidolite sulphuric leachate, adjusts pH value of solution=3.5, step (1) saponification is added
P204 carries out abstraction impurity removal, obtains load organic phases and rich lithium raffinate；
(3) load organic phases use 1mol/L H2SO4Solution is stripped, and is obtained the strip liquor of calcic magnesium-ferrum-aluminum and is stripped organic
Phase, calcium, magnesium, iron, aluminium extraction removal efficiency be respectively 99.2%, 98.8%, 99.8% and 97.9%, the back extraction of calcic magnesium-ferrum-aluminum
Liquid is sent into waste water treatment system, and organic phase is washed for back extraction, non-sodium saponification process in return to step (1) is returned after saponification uses again；
(4) rich lithium raffinate, into bipolar membrane electrodialysis system, obtains a concentration of after depth oil removal treatment in alkali room
The lithium hydroxide solution of 1.5mol/L obtains the sulfuric acid solution of a concentration of 0.75mol/L, sulfuric acid solution return to step in sour room
(3) load organic phases are stripped in；
(5) lithium hydroxide solution that step (4) obtains is handled through evaporation and concentration, obtains concentrated mother liquor (LiOH a concentration of 20
~130g/L) and industrial stage monohydrate lithium hydroxide powder, the rate of recovery of Li is 98.1%；Soap in concentrated mother liquor return to step (1)
Change processing organic extractant.
Embodiment 2：
A method of the high efficiente callback lithium from containing lithium more metal mixed solution includes the following steps：
(1) concentrated mother liquor of output is directly entered the progress of soap tank first order mixing chamber in the step of using embodiment 1 (5)
O/A=1 is compared in saponification process P203+P507+P229 mixed extractants, saponification:1, incorporation time 5min, settling time are
20min, 4 grades of saponification series, organic phase saponification rate are 56%, and the saponification extraction raffinate of soap tank afterbody clarifying chamber enters following steps
Suddenly it is evaporated concentration in (5)；
(2) lithium hydroxide solution of step (4) output in embodiment 1 is added into spodumene sulphuric leachate, adjusts molten
Liquid pH=5.5, the extracting mixed extractant that step (1) saponification process is added detach impurity, obtain load organic phases and rich lithium extracts
Extraction raffinate；
(3) load organic phases use the H of step (4) output in embodiment 12SO4Solution is stripped, and is obtained containing Al, Ca, Mg etc.
The strip liquor of impurity, and it is directly entered waste water treatment system, it is stripped saponification in organic phase return to step (1) and uses again；
(4) rich lithium raffinate, into bipolar membrane electrodialysis system, obtains a concentration of after depth oil removal treatment in alkali room
The lithium hydroxide solution of 2mol/L, obtains the sulfuric acid solution of a concentration of 1mol/L in sour room, right in sulfuric acid solution return to step (3)
Load organic phases are stripped；
(5) lithium hydroxide solution that step (4) obtains is handled through evaporation and concentration, obtains LiOH concentrated mother liquors and technical grade list
The rate of recovery of water lithium hydroxide powder, Li is 96.1%.
Embodiment 3：
A method of the high efficiente callback lithium from containing lithium more metal mixed solution includes the following steps：
(1) 923 mixed extractants of P204+Cyanex 301+Cyanex, using step (5) output in embodiment 2
LiOH concentrated mother liquors carry out saponification process, and O/A=1 is compared in saponification:1.5, incorporation time 8min, settling time 15min, soap
Change 6 grades of series, organic phase saponification rate is 70%, and the saponification extraction raffinate of soap tank afterbody clarifying chamber enters in following step (5)
It is evaporated concentration；
(2) the LiOH solution that step (4) output in embodiment 2 is added in the old halogen of potassium is carried to salt lake, adjusts the pH=of solution
4.8, the extracting mixed extractant separating magnesium of step (1) saponification process is added, obtains load organic phases and rich lithium raffinate；
(3) load organic phases are stripped using HCl solution, obtain magnesium chloride containing solution, and follow-up alternative recycling magnesium is simultaneously made
Standby high purity magnesium hydroxide product is stripped saponification in organic phase return to step (1) and uses again；
(4) rich lithium raffinate, into bipolar membrane electrodialysis system, obtains a concentration of after depth oil removal treatment in alkali room
The lithium hydroxide solution of 3.6mol/L obtains the hydrochloric acid solution of a concentration of 1.8mol/L in sour room, and hydrochloric acid solution can return to step
(3) load organic phases are stripped in；
(5) lithium hydroxide solution that step (4) obtains is handled through evaporation and concentration, obtains industrial stage monohydrate lithium hydroxide powder
The rate of recovery of material, Li is 95.4%.
Claims (9)
1. a kind of method of the high efficiente callback lithium from containing lithium more metal mixed solution, which is characterized in that include the following steps：
(1) pH to 3-7 for adjusting more metal mixed solution containing lithium, then uses saponification organic phase extracting, obtains load organic phases
With rich lithium raffinate；
(2) the load organic phases acid adding back extraction processing, obtains strip liquor and back extraction organic phase；The strip liquor is according to wherein golden
Belong to ionic species and content, selective recovery utilizes, back extraction organic phase is washed, after saponification back to recycling in step (1)；
(3) the rich lithium raffinate enters bipolar membrane electrodialysis system after depth oil removal treatment, output lithium hydroxide solution and
Acid solution；
(4) lithium hydroxide solution obtains monohydrate lithium hydroxide powder and concentrated mother liquor through being concentrated by evaporation.
2. the method as described in claim 1, which is characterized in that the saponification organic phase in step (1) refers to organic phosphates extraction
The organic phase that agent obtains after non-sodium saponification process.
3. method as claimed in claim 2, which is characterized in that the organic phosphates extractant be selected from P204, P507, P229,
At least one of Cyanex272, Cyanex301, Cyanex471X, Cyanex921, Cyanex923.
4. method as claimed in claim 2, which is characterized in that the saponification agent used in the non-soda soap processing procedure is sulphur
It is one or more in the concentrated mother liquor generated in sour lithium, lithium hydroxide, lithium bicarbonate, lithium chloride and step (4).
5. method as claimed in claim 2, which is characterized in that the concentrated mother liquor of step (4) output is directly entered soap tank
First order mixing chamber, the saponification extraction raffinate of soap tank afterbody clarifying chamber, which returns in step (4), is evaporated concentration.
6. method as claimed in claim 2, which is characterized in that in the non-soda soap processing procedure, saponification is comparably O/A=
1:1~1:10, incorporation time is 1~10min, and settling time is 1~30min, 2~10 grades of saponification series.
7. the method as described in claim 1, which is characterized in that in the step (1), solution pH adjusting agent be lithium hydroxide,
It is one or more in sulfuric acid, hydrochloric acid.
8. the method as described in claim 1, which is characterized in that in the step (1), solution pH adjusting agent is in step (3)
The lithium hydroxide solution or acid solution of output.
9. such as method according to any one of claims 1 to 8, which is characterized in that the acid solution of output returns to step in step (3)
Suddenly the back extraction of load organic phases is used in (2).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109097569A (en) * | 2018-09-19 | 2018-12-28 | 江西南氏锂电新材料有限公司 | Utilize the method for calcium, magnesium addition in extraction process removal lithium ore leachate |
| CN111363919A (en) * | 2020-04-03 | 2020-07-03 | 郑州天一萃取科技有限公司 | Compound extracting agent for deep purification of lithium ore leaching solution and purification process |
| CN111394745A (en) * | 2020-03-25 | 2020-07-10 | 意定(上海)信息科技有限公司 | Method for preparing lithium hydroxide from lithium-containing low-magnesium brine |
| WO2020248171A1 (en) * | 2019-06-12 | 2020-12-17 | 中能实用小微科学科技有限公司 | Method for extraction of high-purity lithium with low energy consumption by means of multi-stage recovery |
| CN113003589A (en) * | 2021-04-25 | 2021-06-22 | 湖南金源新材料股份有限公司 | Method for extracting and preparing battery-grade lithium carbonate from P507 raffinate and extraction device |
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| CN107298450A (en) * | 2016-08-31 | 2017-10-27 | 江苏力泰锂能科技有限公司 | The method that lithium hydroxide and lithium carbonate are prepared using soluble lithium salt solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109097569A (en) * | 2018-09-19 | 2018-12-28 | 江西南氏锂电新材料有限公司 | Utilize the method for calcium, magnesium addition in extraction process removal lithium ore leachate |
| WO2020248171A1 (en) * | 2019-06-12 | 2020-12-17 | 中能实用小微科学科技有限公司 | Method for extraction of high-purity lithium with low energy consumption by means of multi-stage recovery |
| CN111394745A (en) * | 2020-03-25 | 2020-07-10 | 意定(上海)信息科技有限公司 | Method for preparing lithium hydroxide from lithium-containing low-magnesium brine |
| CN111363919A (en) * | 2020-04-03 | 2020-07-03 | 郑州天一萃取科技有限公司 | Compound extracting agent for deep purification of lithium ore leaching solution and purification process |
| CN113003589A (en) * | 2021-04-25 | 2021-06-22 | 湖南金源新材料股份有限公司 | Method for extracting and preparing battery-grade lithium carbonate from P507 raffinate and extraction device |
| WO2022228233A1 (en) * | 2021-04-25 | 2022-11-03 | 湖南金源新材料股份有限公司 | Method for extracting and preparing battery-grade lithium carbonate from p507 raffinate, and extraction device |
| CN113003589B (en) * | 2021-04-25 | 2023-04-25 | 湖南金源新材料股份有限公司 | Method and extraction device for extracting and preparing battery grade lithium carbonate from P507 raffinate |
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